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Int. J. Mol. Sci. 2009, 10(11), 4977-4989; doi:10.3390/ijms10114977

Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications?

Inorganic Materials Science, Faculty of Science & Technology, and Mesa+ Research Institute for Nanotechnology, University of Twente, P.O. Box 217, 7500 AE Enschede, The Netherlands
Department of Chemistry, SLU, Box 7015, 75007 Uppsala, Sweden
Author to whom correspondence should be addressed.
Received: 12 October 2009 / Revised: 28 October 2009 / Accepted: 9 November 2009 / Published: 13 November 2009
(This article belongs to the Special Issue Sol-Gel Technique)
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Modification of different zirconium propoxide precursors with H2dea was investigated by characterization of the isolated modified species. Upon modification of zirconium n-propoxide and [Zr(OnPr)(OiPr)3(iPrOH)]2 with ½ a mol equivalent of H2dea the complexes [Zr2(OnPr)6(OCH2CH2)2NH]2 (1) and [Zr2(OnPr)2(OiPr)4(OCH2CH2)2NH]2 (2) were obtained. However, 1H-NMR studies of these tetranuclear compounds showed that these are not time-stable either in solution or solid form. The effect of this time instability on material properties is demonstrated by light scattering and TEM experiments. Modification of zirconium isopropoxide with either ½ or 1 equivalent mol of H2dea results in formation of the trinuclear complex, Zr{η3μ2-NH(C2H4O)2}3[Zr(OiPr)3]2(iPrOH)2 (3) countering a unique nona-coordinated central zirconium atom. This complex 3 is one of the first modified zirconium propoxide precursors shown to be stable in solution for long periods of time. The particle size and morphology of the products of sol-gel synthesis are strongly dependent on the time factor and eventual heat treatment of the precursor solution. Reproducible sol-gel synthesis requires the use of solution stable precursors.
Keywords: precursor chemistry; molecular structure; nona-coordinated zirconium precursor chemistry; molecular structure; nona-coordinated zirconium
This is an open access article distributed under the Creative Commons Attribution License (CC BY 3.0).

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Spijksma, G.I.; Blank, D.H.A.; Bouwmeester, H.J.M.; Kessler, V.G. Modification of Different Zirconium Propoxide Precursors by Diethanolamine. Is There a Shelf Stability Issue for Sol-Gel Applications? Int. J. Mol. Sci. 2009, 10, 4977-4989.

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